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Lithium iron carbonate material prepared by vacuum carbon reduction and method

A lithium iron phosphate, vacuum technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry and other directions, can solve the problems of low bulk density, poor electrical conductivity, increased production cost, etc., to simplify the synthesis process, shorten the reaction time, The effect of improving production efficiency

Inactive Publication Date: 2007-11-14
HUBEI UEE ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0007] Currently, LiFePO 4 The preparation method mainly contains solid phase reaction method, liquid phase method (co-precipitation method, hydrothermal method, sol-gel method and emulsion method etc.), the common feature of all existing methods is exactly the high-purity inert gas that needs flow or high Pure nitrogen protection, flowing inert gas protection technology greatly increases the synthesis cost of lithium iron phosphate
Moreover, due to the incompleteness of all existing synthesis technologies, the consistency of the obtained lithium iron phosphate products is poor, that is to say, the physical and chemical uniformity of the products synthesized by different batches is poor, and the electrochemical performance is inconsistent. further increase its production cost
In addition, lithium iron phosphate also has its own inherent disadvantages, mainly because its bulk density is low, and its theoretical density is 3.6g / cm 3 , its actual tap density is generally only 1.6-1.8g / cm 3
Moreover, lithium iron phosphate is a semiconductor material with poor conductivity.
The existing immature synthesis technology of lithium iron phosphate and the inherent shortcomings of lithium iron phosphate have seriously hindered the large-scale industrial production process of lithium iron phosphate, and also affected the application of lithium iron phosphate materials in various types of lithium ion batteries, especially lithium iron phosphate. Wide application in the field of ion power battery manufacturing

Method used

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  • Lithium iron carbonate material prepared by vacuum carbon reduction and method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In the first step, ferric phosphate, lithium hydroxide, and aluminum dihydrogen phosphate are mixed in a ratio of 1:1:1:0.05 in a molar ratio of P:Fe:Li:Al;

[0030] In the second step, the above mixture is placed in a vacuum high-energy ball mill jar and vacuumized to 10 -2 Pa, ball milled for 12 hours;

[0031] In the third step, the carbon reducing agent activated carbon is added to the above-mentioned ball-milled mixture in the ratio of Fe: C molar ratio of 1: 0.8, and vacuumized to 10 -2 Pa, continue ball milling for 6 hours to obtain a reaction precursor;

[0032] The fourth step is to transfer the above-mentioned reactant precursor to the vacuum reaction furnace, pass high-purity nitrogen gas for 5 minutes, and then vacuumize to 10 -2 Pa, heating, controlling the temperature to 450°C, keeping the furnace temperature constant for 24 hours, passing high-purity nitrogen gas for 45 minutes, sealing and cooling to room temperature, and obtaining carbon-coated alumin...

Embodiment 2

[0035] In the first step, ferrous phosphate and lithium phosphate, doped metal compound aluminum dihydrogen phosphate, zinc oxide, magnesium oxide, and cobalt oxide are mixed according to P: Fe: Li: M (M represents doped metal, Al: Zn: Mg: Co Molar ratio is 1: 1: 1: 0.5) and the molar ratio is 1: 1: 1: 0.03 ratio mixing;

[0036] In the second step, the above mixture is placed in a vacuum high-energy ball mill jar and vacuumized to 10 -3 Pa, ball milled for 10 hours;

[0037] In the third step, the carbon reducing agent acetylene black and graphite (ratio of 1:1) are added to the above-mentioned treated mixture in the ratio of Fe:C molar ratio of 1:1, and vacuumized to 10 -3 Pa, continue ball milling for 8 hours to obtain a reaction precursor;

[0038] The fourth step is to transfer the above-mentioned reactant precursor to the vacuum reaction furnace, pass high-purity nitrogen gas for 30 minutes, and then vacuumize to 10 -3 Pa, heat, control the temperature at 650°C, keep ...

Embodiment 3

[0041] The first step mixes ferrous phosphate with lithium phosphate and zinc oxide in a ratio of 1:1:1:0.02 in the molar ratio of P:Fe:Li:Zn;

[0042] In the second step, the above mixture is placed in a vacuum high-energy ball mill jar and vacuumized to 10 -2 Pa, ball milled for 11 hours;

[0043] In the third step, the carbon reducing agent graphite is added to the above-mentioned ball-milled mixture in the ratio of Fe: C molar ratio of 1: 1.4, and vacuumized to 10 -2 Pa, continue ball milling for 9 hours to obtain a reaction precursor;

[0044] The fourth step is to transfer the above-mentioned reactant precursor to the vacuum reaction furnace, pass high-purity nitrogen gas for 5 minutes, and then vacuumize to 10 -2 Pa, heat, control the temperature at 550°C, keep the furnace temperature constant for 20 hours, pass high-purity nitrogen gas for 45 minutes, seal and cool to room temperature, and obtain metal aluminum-doped lithium iron phosphate powder coated with carbon. ...

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Abstract

This invention relates to a kind of anode material and method used for reducing preparation of lithium iron phosphate by vacuum carbon. It uses cheap phosphate, iron compound and lithium compound as raw material, compound of cheap heavy metal as adulteration modifying agent, cheap and abundant activated carbon, acetylene black and graphite as reducing agent. Dealing with it using ball milling techniques and makes solid-phase chemical reaction under the vacuum condition, then get the anode material adulterating lithium iron phosphate which contains carbon. Lithium iron phosphate compounded in this invention has a stable performance, physical chemistry of products has a good homogeneity and consistency and a high productivity; lithium iron phosphate produced in this invention has a high tap density and electric specific votume, good discharging capability of high-current, stable electrochemistry circulation capability, and low local action, besides, it is easy to control content of tantalum adulterated. The tap density of lithium iron phosphate produced by this method is 1.63-2.04g / cu cm, the highest discharging specific votume is 161.3mAh / g.

Description

technical field [0001] The invention relates to the technical field of preparation of lithium ion battery materials, in particular to a lithium iron phosphate cathode material prepared by vacuum carbon reduction and a preparation method thereof. Background technique [0002] Lithium-ion battery is a new generation of green high-energy battery, which has many excellent characteristics such as high working voltage, high energy density, good electrochemical cycle performance, small self-discharge, no memory effect, and wide actual working temperature range. Therefore, since commercial production in 1992, lithium-ion batteries have been widely used in mobile phones, mobile computers, digital cameras, digital cameras, electronic instruments, military portable equipment, etc. Entering the 21st century, especially in the past five years, the lithium-ion battery industry has developed rapidly, and the output of lithium-ion batteries has also increased rapidly, and its application fi...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 周环波库宗军周亚洲龚春丽丁瑜葛杏莉
Owner HUBEI UEE ENERGY TECH CO LTD
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